Abstract: The common determination method of sulfur content in the collaborative disposal of hazardous waste distillation residue in cement kilns has some problems, such as complicated operation, low sensitivity, high test conditions, and serious environmental pollution. The method of “oxygen bomb combustion-ion chromatography” is used to determine the sulfur content in the distillation residue, which overcomes the deficiency of the conventional detection method and improves the accuracy and reproducibility of the detection results. The sulfur content analysis and detection experiment showed that under the oxygen bomb combustion pressure of 3.0MPa, the absorption liquid is 0.5mol/L NaOH solution, the action time of the absorption liquid is 20min, and the mobile phase flow rate of 100mL/min, the mass concentration of sulfate showed a good linear relationship in the range of 0.5~50mg/L, the correlation coefficient >0.999, the average recovery of spiking (adding standard solution) was 96.8%.